CN104865232B - Method for selectively detecting ascorbic acid by utilizing metal-organic framework material - Google Patents
Method for selectively detecting ascorbic acid by utilizing metal-organic framework material Download PDFInfo
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- CN104865232B CN104865232B CN201510272995.1A CN201510272995A CN104865232B CN 104865232 B CN104865232 B CN 104865232B CN 201510272995 A CN201510272995 A CN 201510272995A CN 104865232 B CN104865232 B CN 104865232B
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Abstract
The invention discloses a method for selectively detecting ascorbic acid by utilizing a metal-organic framework material. The method comprises the following steps: adding 400 [mu]L of a Tris-HCl buffer solution (0.1 M), 5-2000 [mu]L of ascorbic acid (2 mM) and 200-2000 [mu]L of a metal-organic framework material suspension liquid (200 mg/L＜-1＞) in sequence; adding water till the constant volume reaches 4 mL, standing for 5-15 minutes, measuring the fluorescence emission spectrum of a reaction system after the reaction system is stabilized, and calculating the concentration of ascorbic acid in a liquid to be measured through the strength and the linear equation of the fluorescence emission spectrum. The method provided by the invention has a relatively wide detection range and a relatively low detection limit, the process for detecting ascorbic acid is simple and easy to operate, and the method is beneficial for popularization in future.
Description
This patent is subject to state natural sciences fund general project 21375095, National Outstanding Ph.D. Dissertation author special
Item subsidizes fund FANEDD-201023, Tianjin applied basic research plan key project 12JCZDJC21700 and Tianjin
The subsidy of " 131 " innovative talent cultivation engineering the first hierarchical item ZX110185.Tianjin application foundation grinds with cutting edge technology
Study carefully the money of plan Tianjin Nsfc Projects 14JCQNJC05900 and project of national nature science fund project 21301128
Help.
Technical field
The invention belongs to metal-organic framework materials preparing technical field, and in particular to a kind of metal-organic framework materials pair
The detection method of ascorbic acid.
Background technology
Metal-organic framework materials（Metal-Organic Frameworks, MOFs) be a class by metal ion/
The framework material that cluster body is formed by coordinate bond with nitrogenous, oxygen aromatic acid or the multiple tooth organic ligand self assembly of alkali, and quilt
Referred to as Porous coordination polymer（Porous coordination polymer, PCP）.Metal-organic framework materials have novelty
Topological structure, the specific surface area of super large and good heat stability so that this kind of material is stored in gas, catalysis, medicine delay
Release, molecule sensing, imaging etc. aspect have a wide range of applications.
Ascorbic acid is a kind of important antioxidant, and important effect is play in the diet of our mankind,
Additionally, ascorbic acid can also be used to prevent and treat common cold, mental sickness, sterility and infertility, the disease such as acquired immune deficiency syndrome (AIDS) and cancer.
In recent years, as increasing chemical material is found, detect that also layer goes out for the method for ascorbic acid using these materials
It is not poor.The method of traditional detection ascorbic acid has gas chromatography, high performance liquid chromatography, electrochemical process, ultra-violet absorption spectrum
Method etc..There is detection time length, detection process complexity, expensive equipment, the low deficiency of detection sensitivity in these methods.
And the excellent optical property of metal-organic framework materials makes it at aspects such as fluoroscopic examination metal ion, nitro explosives
There are many applications, and be applied to fluoroscopic examination ascorbic acid, be rarely reported.This method is using ascorbic acid and the organic bone of metal
Specific Interactions between frame material, using Fluorometric assay ascorbic acid, can be become by reaction system fluorescence emission spectrum
The rapid sensitive detection of Ascorbic Acid is realized in change.
The content of the invention
The present invention is using the excellent optical property of metal-organic framework materials and ascorbic acid and metal-organic framework materials
Between Specific Interactions, using Fluorometric assay ascorbic acid, can by reaction system fluorescence emission spectrum change realize
The rapid sensitive detection of Ascorbic Acid.
For achieving the above object, the invention discloses metal-organic framework materials answering in fluoroscopic examination ascorbic acid
With.The method for detecting ascorbic acid using metal-organic framework materials is also disclosed that simultaneously, and it is to sequentially add 400 L pH=
The Tris-HCl buffer solution (0.1 M) of 6.0-9.6,5-2000 L ascorbic acid (2 mM) and 200-2000 L metals are organic
Framework material suspension (200 mg L-1), add water and be settled to 4 mL, 5-15 minutes are stood, determine anti-after question response stable system
The fluorescence emission spectrum of system is answered, ascorbic acid in prepare liquid is calculated by the intensity and linear equation of fluorescence emission spectrum
Concentration.
The present invention further discloses prepared by the method detected using metal-organic framework materials Ascorbic Acid
Detection human urine, the aspect application of Ascorbic Acid in Blood Serum content.Experimental result shows：Detection method provided by the present invention has
Wider detection range and relatively low detection limit, detection ascorbic acid process is simple, it is easy to operate.
High spot reviews of the present invention：
（1）Application potential of the outstanding luminosity of metal-organic framework materials in terms of fluoroscopic examination；
（2）Application of the metal-organic framework materials in selective enumeration method ascorbic acid；
（3）Metal-organic framework materials are applied to detect human urine, the detection of Ascorbic Acid in Blood Serum；
Currently preferred example is described as follows：
A) metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation：According to document (Y. Y.
Wang, Q. Jin, S. X. Liu, C. Guo, Y. Y. Liu, B. Ding, X. X. Wu, Y. Li, Z. Z.
Zhu, RSC Adv., 2015,5,35238), by Cd (ClO4)2·6H2O (20.9 mg, 0.05 mmol) and 4- (1H-
1,2,4- triazole -1- ylmethyls) aniline (abtz) (17.4 mg, 0.1 mmol) is blended in high purity water (5 mL) and first
In alcohol (5 mL), 0.5 h is stirred, fortnight is dried under room temperature after filtration, obtain clear crystal.By above-mentioned product（0.3565g,
0.5mmol）And NH4SCN（0.076g, 1 mmol）In 10 mL water/methanol（v/v = 1:1）Mix one hour in solution,
Then mixed solution is transferred in teflon-lined autoclave, the h of reacting by heating 12 under conditions of 160 DEG C
Afterwards, the h of natural cooling 72 at ambient temperature.After being washed for several times with water and ether, sucking filtration obtains clear crystal, i.e. { [Cd
(abtz)2(NCS)]·(ClO4)}n。
B) application of metal-organic framework materials prepared by above-mentioned preparation method on detection ascorbic acid：Sequentially add
The Tris-HCl buffer solution (0.1 M) of 400 L pH=6.0-9.6,5-2000 L ascorbic acid (2 mM) and 200-2000
L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, 5-15 minutes are stood, question response system is steady
The fluorescence emission spectrum of reaction system is determined after fixed, is calculated in prepare liquid by the intensity and linear equation of fluorescence emission spectrum
The concentration of ascorbic acid.
Fluorometric assay ascorbic acid approach disclosed by the invention compared with prior art, with following beneficial effect
Really：
（1）Detection method provided by the present invention has wider detection range and a relatively low detection limit, this method and other
Method is relatively shown in Table 1, illustrates that this method has wider detection range and relatively low detection limit；
（2）The present invention is simple using metal-organic framework materials detection ascorbic acid process, it is easy to operate, and fluorescence spectrophotometer
Photometer is more typical：
Conclusion：Illustrate that this method has wider detection range and relatively low detection limit.
Description of the drawings：
Fig. 1 is the powder diagram of metal-organic framework materials, illustrates that this patent has successfully synthesized what is reported in document
Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}n；
Fig. 2 is the ultraviolet spectrogram and fluorescent emission figure of metal-organic framework materials, illustrates the metal synthesized in this patent
Organic framework material has stronger absorption at 250 nm, therefore the use of 250 nm is excitation wavelength, in the excitation wavelength of 250 nm
Under, the metal-organic framework materials of this method synthesis have excitation peak at 348 nm；
Fig. 3 is optimization metal-organic framework materials concentration map, illustrates that in concentration range be 20-100 mg L-1, metal is organic
Framework material fluorescence intensity first gradually rises, and when the concentration is too high, fluorescence intensity is gradually lowered；
Fig. 4 is optimization metal-organic framework materials pH figures, illustrates under the conditions of pH=6.0-9.6, metal-organic framework materials
Fluorescence intensity is without too big change；
Fig. 5 is the fluorescence spectra that metal-organic framework materials detect ascorbic acid, is illustrated with ascorbic acid concentrations
Increase, the fluorescent emission intensity of reaction system gradually lowers；
Fig. 6 be metal-organic framework materials detect ascorbic acid range of linearity figure, illustrate be in ascorbic acid concentrations
In the range of 0.25 M-75 M, the concentration of ascorbic acid is linear with fluorescent quenching intensity in reaction system, its linear side
Cheng Wei：I0- I = 10.8422 + 5.49051C0 , R2=0.9984。
Specific embodiment
By the description for carrying out to its exemplary embodiment below in conjunction with the accompanying drawings, features described above of the present invention and advantage will become
Must become apparent from it is easy to understand.The present invention is described in further detail with reference to instantiation.
Chemical reagent used is at least and analyzes pure, and high purity water is purchased from heartily pure waters corporation, Cd (ClO4)2·6H2O, 4-
(1H-1,2,4- triazole -1- ylmethyls) aniline (abtz), NH4SCN, methanol unify scientific and technological limited public affairs purchased from the Tianjin sky over the river
Department, trishydroxymethylaminomethane（Tris）Purchased from Beijing Ding Guo Bioisystech Co., Ltd, L-AA, glucose, carbamide,
NaCl、KCl、CaCl2、 (CH3COO)2Zn·2H2O is purchased from Tianjin recovery development in science and technology company limited, CH3COONa·3H2O
Purchased from northern day medical chemistry chemical reagent work, glycine is purchased from Tianjin Zhujiang River Sanitary Materials Factory.
Embodiment 1
Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation：According to document (Y. Y. Wang,
Q. Jin, S. X. Liu, C. Guo, Y. Y. Liu, B. Ding, X. X. Wu, Y. Li, Z. Z. Zhu,
RSC Adv., 2015,5,35238), by Cd (ClO4)2·6H2O (20.9 mg, 0.05 mmol) and 4- (1H-1,2,
4- triazole -1- ylmethyls) aniline (abtz) (17.4 mg, 0.1 mmol) is blended in high purity water (5 mL) and methanol
(in 5 mL, 0.5 h is stirred, fortnight is dried under room temperature after filtration, obtain clear crystal.By above-mentioned product（0.3565g,
0.5mmol）And NH4SCN（0.076g, 1 mmol）In 10 mL water/methanol（v/v = 1:1）Mix one hour in solution,
Then mixed solution is transferred in teflon-lined autoclave, the h of reacting by heating 12 under conditions of 160 DEG C
Afterwards, the h of natural cooling 72 at ambient temperature.After being washed for several times with water and ether, sucking filtration obtains clear crystal.Spread out by powder
Figure contrast is penetrated, we successfully synthesize the { [Cd (abtz) of document report2(NCS)]·(ClO4)}n。
Embodiment 2
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1
（2）200 mg L-1The preparation of metal-organic framework materials suspension：20 mg metal-organic framework materials are weighed,
In the volumetric flask of 100 mL, ultrasonic disperse is put in shady place stand-by to constant volume；
（3）0.1 M, the preparation of 25 DEG C of Tris-HCl buffer：Eight parts of Tris 0.01mol, Mr=are weighed respectively
121.14, the NaCl containing 10 mM, in 0.001 molNaCl to eight beaker, be with the hydrochloric acid tune pH of 0.1 M and 5 M respectively
6.0,6.8,7.4,8.2,8.4,8.9,9.3,9.6 constant volumes are put in stand-by in refrigerator in 100mL volumetric flasks；
（3）2 mM ascorbic acid mother liquors：The mol of ascorbic acid 0.04, Mr=176.12 are weighed, constant volume is in 10 mL
In color comparison tube, now with existing system；
Embodiment 3
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1, related solution
Embodiment 2 is shown in preparation
（2）Fluorescence-detecting step：Sequentially add Tris-HCl buffer solution (0.1 M), the 0-2000 of 400 L pH=6.0
L ascorbic acid (2 mM) and 2000 L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, it is quiet
Put 5 minutes, the fluorescence emission spectrum of reaction system is determined after question response stable system.
Embodiment 4
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1, related solution
Embodiment 2 is shown in preparation
（2）Fluorescence-detecting step：Sequentially add Tris-HCl buffer solution (0.1 M), the 0-2000 of 400 L pH=7.4
L ascorbic acid (2 mM) and 2000 L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, it is quiet
Put 5 minutes, the fluorescence emission spectrum of reaction system is determined after question response stable system.
Embodiment 5
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1, related solution
Embodiment 2 is shown in preparation
（2）Fluorescence-detecting step：Sequentially add Tris-HCl buffer solution (0.1 M), the 0-2000 of 400 L pH=8.9
L ascorbic acid (2 mM) and 2000 L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, it is quiet
Put 15 minutes, the fluorescence emission spectrum of reaction system is determined after question response stable system.
Embodiment 6
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1, related solution
Embodiment 2 is shown in preparation
（2）Fluorescence-detecting step：Sequentially add Tris-HCl buffer solution (0.1 M), the 0-2000 of 400 L pH=6.0
L ascorbic acid (2 mM) and 200 L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, stand
15 minutes, the fluorescence emission spectrum of reaction system is determined after question response stable system.
Embodiment 7
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1, related solution
Embodiment 2 is shown in preparation
（2）Fluorescence-detecting step：Sequentially add Tris-HCl buffer solution (0.1 M), the 0-2000 of 400 L pH=7.4
L ascorbic acid (2 mM) and 1200 L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, it is quiet
Put 10 minutes, the fluorescence emission spectrum of reaction system is determined after question response stable system.
Embodiment 8
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1, related solution
Embodiment 2 is shown in preparation
（2）Fluorescence-detecting step：Sequentially add Tris-HCl buffer solution (0.1 M), the 0-2000 of 400 L pH=8.9
L ascorbic acid (2 mM) and 2000 L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, it is quiet
Put 10 minutes, the fluorescence emission spectrum of reaction system is determined after question response stable system.
Embodiment 9
Chaff interference is determined in reaction system：The M of ascorbic acid concentrations 25 has probed into right as standard, respectively with reaction system
Common interference thing carbamide, glucose, glycine, K+、Na+、Ca2+、Zn2+ Capacity of resisting disturbance.
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1, related solution
Embodiment 2 is shown in preparation
（2）The common interference thing carbamide of variable concentrations is prepared respectively（4 mM）, glucose（4 mM）, glycine（4 mM）、K+（100 mM）、Na+（50 mM）、Ca2+（50 mM）、Zn2+（50 mM）Solution.
（3）Sequentially add the Tris-HCl buffer solution (0.1 M) and the organic bone of 1200 L metals of 400 L pH=7.4
Frame material suspension (200 mg L-1), add water and be settled to 4 mL, 10 minutes are stood, determine reactant after question response stable system
The fluorescent emission intensity of system is I0。
（4）Sequentially add Tris-HCl buffer solution (0.1 M), the 50 L ascorbic acid (2 mM) of 400 L pH=7.4
With 1200 L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, 10 minutes are stood, question response body
The fluorescent emission intensity that reaction system is determined after system is stable is I1。
（5）Sequentially add Tris-HCl buffer solution (0.1 M), the 50 L ascorbic acid (2 of 400 L pH=7.4
MM), common interference thing and 1200 L metal-organic framework materials suspensions (200 mg L-1), add water and be settled to 4 mL, stand
10 minutes, the fluorescent emission intensity that reaction system is determined after question response stable system was I2。
By (I1-I2)/(I0-I1) it is less than 5% concentration, it is determined as this kind of chaff interference Cmax that reaction system can bear.
Test result such as table 3, illustrates there is good selectivity, such as table 2 using this method detection ascorbic acid：
Embodiment 10
（1）Metal-organic framework materials { [Cd (abtz)2(NCS)]·(ClO4)}nPreparation see embodiment 1, related solution
Embodiment 2 is shown in preparation
（4）Urine, blood serum sample be collected from health volunteer, urine, blood serum sample through 5000 rotating speeds, at centrifugation
Reason is stand-by after 10 minutes.Sequentially add Tris-HCl buffer solution (0.1 M), the 40-100 L urines of 400 L pH=7.4
Or serum, 0-10 L ascorbic acid (2 mM) and 1200 L metal-organic framework materials suspensions (200 mg L-1), add water
4 mL are settled to, 10 minutes are stood, the fluorescence emission spectrum of reaction system are determined after question response stable system, by fluorescent emission
The intensity of spectrum and linear equation calculate the concentration of ascorbic acid in prepare liquid, the result such as table 3 of detection：
Illustrate that this method can be used for the high selectivity detection of ascorbic acid in actual sample.
Claims (2)
1. a kind of method that employing metal-organic framework materials Ascorbic Acid is detected, it is characterised in that：Sequentially add 400
The Tris-HCl buffer solution of L pH=6.0-9.6, concentration is 0.1 M；5-2000 L ascorbic acid, its concentration is 2 mM；
200-2000 L metal-organic framework materials suspensions, its weight is 200 mg L-1, add water and be settled to 4 mL, stand 5-15 point
Clock, determines the fluorescence emission spectrum of reaction system after question response stable system, the intensity and linear side by fluorescence emission spectrum
Journey calculates the concentration of ascorbic acid in prepare liquid；Described metal-organic framework materials are referred to：[Cd(abtz)2
(NCS)]·ClO4。
2. the method for being detected using metal-organic framework materials Ascorbic Acid described in claim 1 is detecting Human Urine
Liquid, the aspect application of Ascorbic Acid in Blood Serum content.
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| CN106018360B (en) * | 2016-05-13 | 2018-07-17 | 深圳职业技术学院 | A method of urea is detected based on metal-organic framework materials fluorescent optical sensor |
| CN107664630B (en) * | 2016-07-30 | 2020-01-07 | 天津师范大学 | Dopamine detection method based on metal organic framework material |
| CN109239037B (en) * | 2018-09-28 | 2021-03-26 | 长沙理工大学 | Biosensor based on MOFs as energy receptor and preparation method and application thereof |
| CN109632750A (en) * | 2019-01-07 | 2019-04-16 | 天津师范大学 | A method of dichromate ion is detected using metal-organic framework materials |
| CN110987893B (en) * | 2019-12-30 | 2022-04-26 | 福建师范大学 | Method for quantitatively detecting ascorbic acid |
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